#------------------------------------------------------------------------------
#$Date: 2020-10-06 11:44:47 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257530 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/47/7704789.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7704789
loop_
_publ_author_name
'Yao, Zhi-Yuan'
'Zhang, Guo-Qin'
'Yao, Wan-Wan'
'Wang, Xiao-Zu'
'Qian, Yin'
'Ren, Xiao-Ming'
_publ_section_title
;
 Uniaxial thermal expansion behaviors and ionic conduction in a layered
 (NH₄)₂V₃O₈.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10638
_journal_page_last               10644
_journal_paper_doi               10.1039/d0dt01833c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '0.5(O16 V6), H8 N2'
_chemical_formula_sum            'H8 N2 O8 V3'
_chemical_formula_weight         316.90
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_Hall           'P 4 -2ab'
_space_group_name_H-M_alt        'P 4 b m'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2019-12-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-20 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8891(3)
_cell_length_b                   8.8891(3)
_cell_length_c                   5.5691(5)
_cell_measurement_reflns_used    2583
_cell_measurement_temperature    270(2)
_cell_measurement_theta_max      27.438
_cell_measurement_theta_min      4.586
_cell_volume                     440.05(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      270.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4274
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.436
_diffrn_reflns_theta_min         3.241
_exptl_absorpt_coefficient_mu    3.138
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1195 before and 0.0769 after correction. The Ratio of minimum to maximum transmission is 0.7659. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.392
_exptl_crystal_description       plate
_exptl_crystal_F_000             310
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Flack x determined using 224 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         556
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+1.7111P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0697
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                527
_reflns_number_total             556
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01833c2.cif
_cod_data_source_block           270k-1
_cod_depositor_comments
;Adding full bibliography for 7704781--7704792.cif.

 Adding full bibliography for 7704781--7704792.cif.
;
_cod_original_cell_volume        440.05(5)
_cod_database_code               7704789
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.17(10)
 0.83(10)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H,H) groups
3. Restrained distances
 N1-H1D
 0.9 with sigma of 0.02
4. Others
 Fixed Sof: H1B(0.5) H1C(0.5)
5.a Riding coordinates:
 N1(H1A,H1B,H1C), N1(H1D)
;
_shelx_res_file
;
    270k-1.res created by SHELXL-2014/7

TITL 270K-1 in P4bm
CELL 0.71073 8.8891 8.8891 5.5691 90 90 90
ZERR 2 0.0003 0.0003 0.0005 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,+Z
SYMM 0.5-Y,0.5-X,+Z
SYMM 0.5+Y,0.5+X,+Z
SFAC H N O V
UNIT 16 4 16 6
DFIX 0.9 N1 H1d

L.S. 4
PLAN  1
TEMP -3.15
CONF
MORE -1
BOND $H
fmap 2
acta
TWIN 1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\270K-1.hkl">
REM </olex2.extras>

WGHT    0.000000    1.711100
BASF   0.83252
FVAR       0.26554
V2    4   -0.633518   -0.133518   -0.214158    10.50000    0.00804    0.00804 =
         0.01545    0.00063    0.00063    0.00039
O4    3   -0.630335   -0.130335   -0.507868    10.50000    0.02407    0.02407 =
         0.01181   -0.00198   -0.00198   -0.00598
O3    3   -0.500000    0.000000   -0.099988    10.25000    0.01594    0.01594 =
         0.01864    0.00000    0.00000   -0.00624
O2    3   -0.807083   -0.085683   -0.107065    11.00000    0.01076    0.01845 =
         0.03388    0.00274    0.00204    0.00545
V1    4   -1.000000    0.000000   -0.210635    10.25000    0.00889    0.00889 =
         0.01753    0.00000    0.00000    0.00000
O1    3   -1.000000    0.000000   -0.496810    10.25000    0.03435    0.03435 =
         0.01660    0.00000    0.00000    0.00000
N1    2   -0.830601   -0.330601   -0.744279    10.50000    0.03176    0.03176 =
         0.01944   -0.00042   -0.00042   -0.01202
AFIX   3
H1A   1   -0.820571   -0.320470   -0.902479    10.50000   -1.20000
H1B   1   -0.809171   -0.424070   -0.702229    10.50000   -1.20000
H1C   1   -0.924781   -0.308460   -0.702229    10.50000   -1.20000
AFIX   3
H1D   1   -0.766461   -0.266360   -0.668539    10.50000   -1.20000
AFIX   0
HKLF 4

REM  270K-1 in P4bm
REM R1 =  0.0325 for     527 Fo > 4sig(Fo)  and  0.0358 for all     556 data
REM     39 parameters refined using      2 restraints

END

WGHT      0.0000      1.4949

REM Highest difference peak  0.509,  deepest hole -0.491,  1-sigma level  0.101
Q1    1  -0.6121 -0.0356 -0.2131  11.00000  0.05    0.51
;
_shelx_res_checksum              57183
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V -0.63352(8) -0.13352(8) -0.2142(4) 0.0105(3) Uani 1 2 d S T P . .
O4 O -0.6303(5) -0.1303(5) -0.5079(11) 0.0200(13) Uani 1 2 d S T P . .
O3 O -0.5000 0.0000 -0.1000(14) 0.0168(17) Uani 1 4 d S T P . .
O2 O -0.8071(5) -0.0857(5) -0.1071(9) 0.0210(9) Uani 1 1 d . . . . .
V1 V -1.0000 0.0000 -0.2106(5) 0.0118(3) Uani 1 4 d S T P . .
O1 O -1.0000 0.0000 -0.4968(17) 0.028(2) Uani 1 4 d S T P . .
N1 N -0.8306(5) -0.3306(5) -0.7443(18) 0.0277(19) Uani 1 2 d DS T P . .
H1A H -0.8206 -0.3205 -0.9025 0.033 Uiso 1 2 d RS T P . .
H1B H -0.8092 -0.4241 -0.7022 0.033 Uiso 0.5 1 d R . . . .
H1C H -0.9248 -0.3085 -0.7022 0.033 Uiso 0.5 1 d R . . . .
H1D H -0.7665 -0.2664 -0.6685 0.033 Uiso 1 2 d DRS T P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V2 0.0080(3) 0.0080(3) 0.0155(5) 0.0006(7) 0.0006(7) 0.0004(4)
O4 0.024(2) 0.024(2) 0.012(3) -0.0020(17) -0.0020(17) -0.006(3)
O3 0.016(2) 0.016(2) 0.019(4) 0.000 0.000 -0.006(3)
O2 0.011(2) 0.018(2) 0.034(2) 0.0027(18) 0.0020(18) 0.0054(17)
V1 0.0089(4) 0.0089(4) 0.0175(8) 0.000 0.000 0.000
O1 0.034(3) 0.034(3) 0.017(5) 0.000 0.000 0.000
N1 0.032(2) 0.032(2) 0.019(5) 0.000(2) 0.000(2) -0.012(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 V2 O3 109.3(3) . . ?
O4 V2 O2 111.1(2) . 8_455 ?
O4 V2 O2 111.1(2) . . ?
O2 V2 O3 108.0(2) . . ?
O2 V2 O3 108.0(2) 8_455 . ?
O2 V2 O2 109.1(3) . 8_455 ?
V2 O3 V2 138.5(5) . 2_455 ?
V2 O2 V1 141.5(3) . . ?
O2 V1 O2 85.05(9) 4_445 . ?
O2 V1 O2 85.05(9) 4_445 2_355 ?
O2 V1 O2 145.8(3) 3_465 4_445 ?
O2 V1 O2 145.8(3) 2_355 . ?
O2 V1 O2 85.05(9) 3_465 2_355 ?
O2 V1 O2 85.05(9) 3_465 . ?
O1 V1 O2 107.09(16) . . ?
O1 V1 O2 107.09(16) . 4_445 ?
O1 V1 O2 107.09(16) . 3_465 ?
O1 V1 O2 107.09(16) . 2_355 ?
H1A N1 H1B 109.6 . . ?
H1A N1 H1C 109.4 . . ?
H1A N1 H1D 109.4 . . ?
H1B N1 H1C 109.9 . . ?
H1B N1 H1D 109.4 . . ?
H1C N1 H1D 109.1 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V2 O4 1.636(6) . ?
V2 O3 1.795(3) . ?
V2 O2 1.708(4) 8_455 ?
V2 O2 1.708(4) . ?
O3 V2 1.795(3) 2_455 ?
O2 V1 1.963(4) . ?
V1 O2 1.963(4) 4_445 ?
V1 O2 1.963(4) 2_355 ?
V1 O2 1.963(4) 3_465 ?
V1 O1 1.594(9) . ?
N1 H1A 0.8901 . ?
N1 H1B 0.8840 . ?
N1 H1C 0.8913 . ?
N1 H1D 0.9105 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 V2 O3 V2 0.000(0) . . . 2_455 ?
O4 V2 O2 V1 -11.9(5) . . . . ?
O3 V2 O2 V1 108.0(5) . . . . ?
O2 V2 O3 V2 -121.0(2) . . . 2_455 ?
O2 V2 O3 V2 121.0(2) 8_455 . . 2_455 ?
O2 V2 O2 V1 -134.8(3) 8_455 . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.17(10)
2 0.83(10)
